High purity tantalum, products containing the same, and methods of making the same

ABSTRACT

High purity tantalum metals and alloys containing the same are described. The tantalum metal preferably has a purity of at least 99.995% and more preferably at least 99.999%. In addition, tantalum metal and alloys thereof are described, which either have a grain size of about 50 microns or less, or a texture in which a (100) intensity within any 5% increment of thickness is less than about 15 random, or an incremental log ratio of (111):(100) intensity of greater than about −4.0, or any combination of these properties. Also described are articles and components made from the tantalum metal which include, but are not limited to, sputtering targets, capacitor cans, resistive film layers, wire, and the like. Also disclosed is a process for making the high purity metal which includes the step of reacting a salt-containing tantalum with at least one compound capable of reducing this salt to tantalum powder and a second salt in a reaction container. The reaction container or liner in the reaction container and the agitator or liner on the agitator are made from a metal material having the same or higher vapor pressure of melted tantalum. The high purity tantalum preferably has a fine and uniform microstructure.

This application is a continuation of prior U.S. patent application Ser.No. 09/199,569 filed Nov. 25, 1998 now U.S. Pat. No. 6,348,113.

BACKGROUND OF THE INVENTION

The present invention relates to metals, in particular tantalum, andproducts made from tantalum as well as methods of making and processingthe tantalum.

In industry, there has always been a desire to form higher purity metalsfor a variety of reasons. With respect to tantalum, higher purity metalsare especially desirable due to tantalum's use as a sputtering targetand its use in electrical components such as capacitors. Thus,impurities in the metal can have an undesirable effect on the propertiesof the articles formed from the tantalum.

When tantalum is processed, the tantalum is obtained from ore andsubsequently crushed and the tantalum separated from the crushed orethrough the use of an acid solution and density separation of the acidsolution containing the tantalum from the acid solution containingniobium and other impurities. The acid solution containing the tantalumis then crystallized into a salt and this tantalum containing salt isthen reacted with pure sodium in a vessel having an agitator typicallyconstructed of nickel alloy material, wherein tungsten or molybdenum ispart of the nickel alloy. The vessel will typically be a double walledvessel with pure nickel in the interior surface. The salt is thendissolved in water to obtain tantalum powder. However, during suchprocessing, the tantalum powder is contaminated by the various surfacesthat it comes in contact with such as the tungsten and/or molybdenumcontaining surfaces. Many contaminants can be volatized duringsubsequent melting, except highly soluble refractory metals (e.g., Nb,Mo, and W). These impurities can be quite difficult or impossible toremove, thus preventing a very high purity tantalum product.

Accordingly, there is a desire to obtain higher purity tantalum productswhich substantially avoid the contaminations obtained during theprocessing discussed above. Also, there is a desire to have a tantalumproduct having higher purity, a fine grain size, and/or a uniformtexture. Qualities such as fine grain size can be an important propertyfor sputtering targets made from tantalum since fine grain size can leadto improved uniformity of thickness of the sputtered deposited film.Further, other products containing the tantalum having fine grain sizecan lead to improved homogeneity of deformation and enhancement of deepdrawability and stretchability which are beneficial in making capacitorscans, laboratory crucibles, and increasing the lethality of explosivelyformed penetrators (EFP's). Uniform texture in tantalum containingproducts can increase sputtering efficiency (e.g., greater sputter rate)and can increase normal anisotropy (e.g., increased deep drawability),in preform products.

SUMMARY OF THE PRESENT INVENTION

A feature of the present invention is to provide a high purity tantalumproduct exhibiting a fine grain structure and/or uniform texture.

Another feature of the present invention is to provide articles,products, and/or components containing the high purity tantalum.

An additional feature of the present invention is to provide processesto make the high purity tantalum product as well as the articles,products and/or components containing the high purity tantalum.

Additional features and advantages of the present invention will be setforth in part in the description which follows, and in part will beapparent from the description, or may be learned by practice of thepresent invention. The objectives and other advantages of the presentinvention will be realized and attained by means of the elements andcombinations particularly pointed out in the description and appendedclaims.

To achieve these and other advantages, and in accordance with thepurpose of the present invention, as embodied and broadly describedherein, the present invention relates to tantalum metal having a purityof at least 99.995% and more preferably at least 99.999%. The tantalummetal preferably has a fine grain structure and/or uniform texture.

The present invention further relates to an alloy or mixture comprisingtantalum, wherein the tantalum present in the alloy or mixture has apurity of at least 99.995% and more preferably at least 99.999%. Thealloy or mixture (e.g., at least the tantalum present in the alloy ormixture) also preferably has a fine grain structure and/or uniformtexture.

The present invention also relates to a high purity tantalum, e.g.,suitable for use as a sputtering target, having a fully recrystallizedgrain size with an average grain size of about 150 μm or less and/orhaving a primary (111)-type texture substantially throughout thethickness of the tantalum and preferably throughout the entire thicknessof the tantalum metal and/or having an absence of strong (100) texturebands within the thickness of the tantalum.

The present invention further relates to manufacturing plate and sheetfrom the above-mentioned tantalum by flat-forging the tantalum,machining into rolling slabs, annealing rolling slabs, rolling intoplate or sheet, then annealing the plate or sheet. Final products suchas sputtering targets can be then machined from the annealed plate orsheet.

The present invention also relates to a sputtering target comprising theabove-described tantalum and/or alloy. The sputtering target can also beformed by radial forging and subsequent round processing to producebillets or slugs, which are then forged and rolled to yield discs, whichcan then be machined and annealed.

The present invention further relates to resistive films and capacitorscomprising the above-described tantalum and/or alloy.

The present invention also relates to articles, components, or productswhich comprise at least in part the above-described tantalum and/oralloy.

Also, the present invention relates to a process of making theabove-described tantalum which involves reacting a salt-containingtantalum with pure sodium or other suitable salt in a reactive containeror pot and an agitator which both are made from or have a linercomprising a metal or alloy thereof which has the same or higher vaporpressure as tantalum at the melting point of tantalum.

The present invention further relates to processing tantalum powder bymelting the tantalum powder in a high vacuum of 10⁻² torr or more. Thepressure above the melt is lower than the vapor pressures of theimpurities existing in the tantalum. Preferably, the melting of thetantalum powder is accomplished by electron beam melting.

It is to be understood that both the foregoing general description andthe following detailed description are exemplary and explanatory onlyand are intended to provide further explanation of the presentinvention, as claimed.

BRIEF DESCRIPTION OF THE DRAWINGS

FIGS. 1(A-B)-11(A-B) are graphs and corresponding data relating totexture gradient (incremental thickness vs. random) and log ratio(111):(100) gradients (incremental thickness vs. Ln (111/100)) of highpurity tantalum plates of the present invention.

DETAILED DESCRIPTION OF THE PRESENT INVENTION

The present invention relates to a tantalum metal having a purity of atleast 99.995%. Preferably, the tantalum metal has a purity of at least99.999% and can range in purity from about 99.995% to about 99.999% ormore. Other ranges include about 99.998% to about 99.999% and from about99.999% to about 99.9992% and from about 99.999% to about 99.9995%. Thepresent invention further relates to a metal alloy which comprises thehigh purity tantalum metal, such as a tantalum based alloy or otheralloy which contains the high purity tantalum as one of the componentsof the alloy.

The impurities that may be present in the high purity tantalum metal areless than or equal to 0.005% and typically comprise other body-centeredcubic (bcc) refractory metals of infinite solubility in tantalum, suchas niobium, molybdenum, and tungsten.

The tantalum metal and alloys thereof containing the tantalum metalpreferably have a texture which is advantageous for particular end uses,such as sputtering. In other words, when the tantalum metal or alloythereof is formed into a sputtering target having a surface and thensputtered, the texture of the tantalum metal in the present inventionleads to a sputtering target which is easily sputtered and, very few ifany areas in the sputtering target resist sputtering. Further, with thetexture of the tantalum metal of the present invention, the sputteringof the sputtering target leads to a very uniform sputtering erosion thusleading to a sputtered film which is therefore uniform as well. It ispreferred that the tantalum having any purity, but preferably a purityof at least about 99.995%, has a grain size of about 150 microns orless. Preferably, the tantalum metal is at least partiallyrecrystallized, and more preferably at least about 80% of the tantalummetal is recrystallized and even more preferably at least about 98% ofthe tantalum metal is recrystallized. Most preferably, the tantalummetal is fully recrystallized.

Also, it is preferred that the tantalum metal have a fine texture. Morepreferably the texture is such that the (100) peak intensity within any5% incremental thickness of the tantalum is less than about 15 random,and/or has a natural log (Ln) ratio of (111):(100) center peakintensities within the same increment greater than about −4.0 (i.e.,meaning, −4.0, −3.0, −2.0, −1.5, −1.0 and so on) or has both the (100)centroid intensity and the ratio. The center peak intensity ispreferably from about 0 random to about 10 random, and more preferablyis from about 0 random to about 5 random. Other (100) centroid intensityranges include, but are not limited to, from about 1 random to about 10random and from about 1 random to about 5 random. Further, the log ratioof (111):(100) center peak intensities is from about −4.0 to about 15and more preferably from about −1.5 to about 7.0. Other suitable rangesof log ratios, include, but are not limited to, about −4.0 to about 10,and from about −3.0 to about 5.0. Most preferably, the tantalum metalhas the desired purity of at least about 99.995% and the preferred grainsize and preferred texture with regard to the (100) incrementalintensity and the (111):(100) ratio of incremental centroid intensities.The method and equipment that can be used to characterize the textureare described in Adams et al., Materials Science Forum, Vol. 157-162(1994), pp. 31-42; Adams et al., Metallurgical Transactions A, Vol 24A,April 1993-No. 4, pp.819-831; Wright et al., International AcademicPublishers, 137 Chaonei Dajie, Beijing, 1996 (“Textures of Material:Proceedings of the Eleventh International Conference on Textures ofMaterials);Wright, Journal of Computer-Assisted Microscopy, Vol. 5, No.3 (1993), all incorporated in their entirety by reference herein.

The high purity tantalum metal of the present invention can be used in anumber of areas. For instance, the high purity tantalum metal can bemade into a sputtering target or into chemical energy (CE) munitionwarhead liner which comprises the high purity metal. The high puritymetal can also be used and formed into a capacitor anode or into aresistive film layer. The tantalum metal of the present invention can beused in any article or component which conventional tantalum is used andthe methods and means of making the various articles or componentscontaining the conventional tantalum can be used equally here inincorporating the high purity tantalum metal into the various articlesor components. For instance, the subsequent processing used in makingsputtering targets, such as the backing plate, described in U.S. Pat.Nos. 5,753,090, 5,687,600, and 5,522,535 can be used here and thesepatents are incorporated in their entirety by reference herein.

Generally, a process that can be used to make the high purity tantalummetal of the present invention involves a refining process, a vacuummelting process, and a thermal mechanical process. In this process oroperation, the refining process involves the steps of extractingtantalum metal preferably in the form a powder from ore containingtantalum and preferably the ore-containing tantalum selected has lowamounts of impurities, especially, low amounts of niobium, molybdenum,and tungsten. More preferably, the amount of niobium, molybdenum, andtungsten is below about 10 ppm, and most preferably is below about 8ppm. Such a selection leads to a purer tantalum metal. After therefining process, the vacuum melting process is used to purge lowmelting point impurities, such as alkyde and transition metals from thetantalum while consolidating the tantalum material into a fully dense,malleable ingot. Then, after this process, a thermal mechanical processcan be used which can involve a combination of cold working andannealing of a tantalum which further ensures that the preferred grainsize and/or preferred texture and uniformity are achieved, if desired.

The high purity tantalum metal preferably may be made by reacting asalt-containing tantalum with at least one agent (e.g., compound orelement) capable of reducing this salt to the tantalum metal and furtherresults in the formation of a second salt in a reaction container. Thereaction container can be any container typically used for the reactionof metals and should withstand high temperatures on the order of about800° C. to about 1,200° C. For purposes of the present invention, thereaction container or the liner in the reaction container, which comesin contact with the salt-containing tantalum and the agent capable ofreducing the salt to tantalum, is made from a material having the sameor higher vapor pressure as tantalum at the melting point of thetantalum. The agitator in the reaction container can be made of the samematerial or can be lined as well. The liner can exist only in theportions of the reaction container and agitator that come in contactwith the salt and tantalum. Examples of such metal materials which canform the liner or reaction container include, but are not limited to,metal-based materials made from nickel, chromium, iron, manganese,titanium, zirconium, hafnium, vanadium, ruthenium, cobalt, rhodium,palladium, platinum, or any combination thereof or alloy thereof as longas the alloy material has the same or higher vapor pressure as themelting point of tantalum metal. Preferably, the metal is a nickel or anickel-based alloy, a chromium or a chromium-based alloy, or an iron oran iron-based alloy. The liner, on the reaction container and/oragitator, if present, typically will have a thickness of from about 0.5cm to about 3 cm. Other thicknesses can be used. It is within the boundsof the present invention to have multiple layers of liners made of thesame or different metal materials described above.

The salt-containing tantalum can be any salt capable of having tantalumcontained therein such as a potassium-fluoride tantalum. With respect tothe agent capable of reducing the salt to tantalum and a second salt inthe reaction container, the agent which is capable of doing thisreduction is any agent which has the ability to result in reducing thesalt-containing tantalum to just tantalum metal and other ingredients(e.g. salt(s)) which can be separated from the tantalum metal, forexample, by dissolving the salts with water or other aqueous sources.Preferably, this agent is sodium. Other examples include, but are notlimited to, lithium, magnesium, calcium, potassium, carbon, carbonmonoxide, ionic hydrogen, and the like. Typically, the second salt whichalso is formed during the reduction of the salt-containing tantalum issodium fluoride. Details of the reduction process which can be appliedto the present invention in view of the present application are setforth in Kirk-Othmer, Encyclopedia of Chemical Technology, 3^(rd)Edition, Vol 22, pp. 541-564, U.S. Pat. Nos. 2,950,185; 3,829,310;4,149,876; and 3,767,456. Further details of the processing of tantalumcan be found in U.S. Pat. Nos. 5,234,491; 5,242,481; and 4,684,399. Allof these patents and publications are incorporated in their entirety byreference herein.

The above-described process can be included in a multi-step processwhich can begin with low purity tantalum, such as ore-containingtantalum. One of the impurities that can be substantially present withthe tantalum is niobium. Other impurities at this stage are tungsten,silicon, calcium, iron, manganese, etc. In more detail, low puritytantalum can be purified by mixing the low purity tantalum which hastantalum and impurities with an acid solution. The low purity tantalum,if present as an ore, should first be crushed before being combined withan acid solution. The acid solution should be capable of dissolvingsubstantially all of the tantalum and impurities, especially when themixing is occurring at high temperatures.

Once the acid solution has had sufficient time to dissolvesubstantially, if not all, of the solids containing the tantalum andimpurities, a liquid solid separation can occur which will generallyremove any of the undissolved impurities. The solution is furtherpurified by liquid-liquid extraction. Methyl isobutyl ketone (MIBK) canbe used to contact the tantalum rich solution, and deionized water canbe added to create a tantalum fraction. At this point, the amount ofniobium present in the liquid containing tantalum is generally belowabout 25 ppm.

Then, with the liquid containing at least tantalum, the liquid ispermitted to crystallize into a salt with the use of vats. Typically,this salt will be a potassium tantalum fluoride salt. More preferably,this salt is K₂TaF₇. This salt is then reacted with an agent capable ofreducing the salt into 1) tantalum and 2) a second salt as describedabove. This compound will typically be pure sodium and the reaction willoccur in a reaction container described above. As stated above, thesecond salt byproducts can be separated from the tantalum by dissolvingthe salt in an aqueous source and washing away the dissolved salt. Atthis stage, the purity of the tantalum is typically 99.50 to 99.99% Ta.

Once the tantalum powder is extracted from this reaction, any impuritiesremaining, including any contamination from the reaction container, canbe removed through melting of the tantalum powder.

The tantalum powder can be melted a number of ways such as a vacuum arcremelt or an electron beam melting. Generally, the vacuum during themelt will be sufficient to remove substantially any existing impuritiesfrom the recovered tantalum so as to obtain high purity tantalum.Preferably, the melting occurs in a high vacuum such as 10⁻⁴ torr ormore. Preferably, the pressure above the melted tantalum is lower thanthe vapor pressures of the metal impurities in order for theseimpurities, such as nickel and iron to be vaporized. The diameter of thecast ingot should be as large as possible, preferably greater than 9½inches. The large diameter assures a greater melt surface to vacuuminterface which enhances purification rates. In addition, the largeingot diameter allows for a greater amount of cold work to be impartedto the metal during processing, which improves the attributes of thefinal products. Once the mass of melted tantalum consolidates, the ingotformed will have a purity of 99.995% or higher and preferably 99.999% orhigher. The electron beam processing preferably occurs at a melt rate offrom about 300 to about 800 lbs. per hour using 20,000 to 28,000 voltsand 15 to 40 amps, and under a vacuum of from about 1×10⁻³ to about1×10⁻⁶ Torr. More preferably, the melt rate is from about 400 to about600 lbs. per hour using from 24,000 to 26,000 volts and 17 to 36 amps,and under a vacuum of from about 1×10⁻⁴ to 1×10⁻⁵ Torr. With respect tothe VAR processing, the melt rate is preferably of 500 to 2,000 lbs. perhour using 25-45 volts and 12,000 to 22,000 amps under a vacuum of2×10⁻² to 1×10⁻⁴ Torr, and more preferably 800 to 1200 lbs. per hour atfrom 30 to 60 volts and 16,000 to 18,000 amps, and under a vacuum offrom 2×10⁻² to 1×10⁻⁴ Torr.

The high purity tantalum ingot can then be thermomechanically processedto produce the high purity tantalum containing product. The fine, andpreferably fully recrystallized, grain structure and/or uniform textureis imparted to the product through a combination of cold and/or warmworking and in-process annealing. The high purity tantalum productpreferably exhibits a uniform texture of mixed or primary (111)throughout its thickness as measured by orientation imaging microscopy(OIM) or other acceptable means. With respect to thermomechanicalprocessing, the ingot can be subjected to rolling and/or forgingprocesses and a fine, uniform microstructure having high purity can beobtained. The high purity tantalum has an excellent fine grain sizeand/or a uniform distribution. The high purity tantalum preferably hasan average recrystallized grain size of about 150 microns or less, morepreferably about 100 microns or less, and even more preferably about 50microns or less. Ranges of suitable average grain sizes include fromabout 25 to about 150 microns; from about 30 to about 125 microns, andfrom about 30 to about 100 microns.

The resulting high purity metal of the present invention, preferably has10 ppm or less metallic impurities and preferably 50 ppm or less O₂, 25ppm or less N₂, and 25 ppm or less carbon. If a purity level of about99.995 is desired, than the resulting high purity metal preferably hasmetallic impurities of about 50 ppm or less, and preferably 50 ppm orless O₂, 25 ppm or less N₂, and 25 ppm or less carbon.

With respect to taking this ingot and forming a sputtering target, thefollowing process can be used. In one embodiment, the sputtering targetmade from the high purity tantalum metal can be made by mechanically orchemically cleaning the surfaces of the tantalum metal, wherein thetantalum metal has a sufficient starting cross-sectional area to permitthe subsequent processing steps described below. Preferably the tantalummetal has a cross-sectional area of at least 9½ inches or more. The nextstep involves flat forging the tantalum metal into one or more rollingslabs. The rolling slab(s) has a sufficient deformation to achievesubstantially uniform recrystallization after the annealing stepimmediately following this step as described below. The rolling slab(s)is then annealed in vacuum and at a sufficient temperature to achieve atleast partial recystallization of the rolling slab(s). Preferredannealing temperatures and times are set forth below and in theexamples. The rolling slab(s) is then subjected to cold or warm rollingin both the perpendicular and parallel directions to the axis of thestarting tantalum metal (e.g., the tantalum ingot) to form at least oneplate. The plate is then subjected to flattening (e.g., level rolling).The plate is then annealed a final time at a sufficient temperature andfor a sufficient time to have an average grain size of equal to or lessthan about 150 microns and a texture substantially void of (100)textural bands. Preferably, no (100) textural bands exist. The plate canthen be mechanically or chemically cleaned again and formed into thesputtering target having any desired dimension. Typically, the flatforging will occur after the tantalum metal is placed in air for atleast about 4 hours at temperatures ranging from ambient to about 370°C. Also, preferably before cold rolling, the rolling slabs are annealedat a temperature (e.g., from about 950° C. to about 1500° C.) and for atime (e.g., from about ½ hour to about 8 hours) to achieve at leastpartial recrystallization of the tantalum metal. Preferably the coldrolling is transverse rolling at ambient temperatures and the warmrolling is at temperatures of less than about 370° C.

With respect to annealing of the tantalum plate, preferably thisannealing is in a vacuum annealing at a temperature and for a timesufficient to achieve complete recrystallization of the tantalum metal.The examples in this application set forth further preferred detailswith respect to this processing.

Another way to process the tantalum metal into sputtering targetsinvolves mechanically or chemically clean surfaces of the tantalum metal(e.g., the tantalum ingot), wherein the tantalum metal has a sufficientstarting cross-sectional area to permit the subsequent processing asdescribed above. The next step involves round forging the tantalum metalinto at least one rod, wherein the rod has sufficient deformation toachieve substantially uniform recrystallization either after theannealing step which occurs immediately after this step or the annealingstep prior to cold rolling. The tantalum rod is then cut into billetsand the surfaces mechanically or chemically cleaned. An optionalannealing step can occur afterwards to achieve at least partialrecrystallization. The billets are then axially forged into preforms.Again, an optional annealing step can occur afterwards to achieve atleast partial recrystallization. However, at least one of the optionalannealing steps or both are done. The preforms are then subjected tocold rolling into at least one plate. Afterwards, the surfaces of theplate(s) can be optionally mechanically or chemically clean. Then, thefinal annealing step occurs to result in an average grain size of about150 microns or less and a texture substantially void of (100) texturalbands, if not totally void of (100) textural bands. The round forgingtypically occurs after subjecting the tantalum metal to temperatures ofabout 370° C. or lower. Higher temperatures can be used which results inincreased oxidation of the surface. Preferably, prior to forging thebillets, the billets are annealed. Also, the preforms, prior to coldrolling can be annealed. Typically, these annealing temperatures will befrom about 900° C. to about 1200° C. Also, any annealing is preferablyvacuum annealing at a sufficient temperature and for a sufficient timeto achieve recrystallization of the tantalum metal.

Preferably, the sputtering targets made from the high purity tantalumhave the following dimensions: a thickness of from about 0.080 to about1.50″, and a surface area from about 7.0 to about 1225 square inches.

The high purity tantalum preferably has a primary or mixed (111)texture, and a minimum (100) texture throughout the thickness of thesputtering target, and is sufficiently void of (100) textural bands.

The present invention will be further clarified by the followingexamples, which are intended to be purely exemplary of the presentinvention.

EXAMPLES Example 1

Numerous sublots of sodium-reduced commercial-grade tantalum powder,each weighing about 200-800 lbs., were chemically analyzed forsuitability as 99.999% Ta feedstock for electron beam melting.Representative samples from each powder lot were analyzed by GlowDischarge Mass Spectrometry (GDMS): powder sublots having combinedniobium (Nb), molybdenum (Mo), and tungsten (W) impurity content lessthan 8 ppm were selected for melting.

The selected Ta powder sublots were then blended in a V-cone blender toproduce a homogeneous 4000 pound powder master lot, which was againanalyzed by GDMS to confirm purity. Next, the powder was coldisostatically pressed (CIP'ed) into green logs approximately 5.5″-6.5″in diameter, each weighing nominally 300 pounds. The pressed logs werethen degassed by heating at 1450° C. for 2 hours at a vacuum level ofabout 10⁻³-10⁻⁵ torr. For this operation, the logs were covered withtantalum sheets to prevent contamination from the furnace elements.

The degassed logs were then side fed into a 1200KW EB furnace and dripmelted at a rate of 400 lbs./hr. into a 10″ water-cooled copper crucibleunder a vacuum less than 10⁻³ torr. Once cooled, the resultingfirst-melt ingot was inverted, hung in the same furnace, and remeltedusing the same EB melting parameters. The 2^(nd) melt ingot was againinverted and remelted a third time, but into a 12″ crucible at a meltrate of 800 lbs./hr.

A sample was taken from the sidewall of the resulting ingot for chemicalanalysis by Glow Discharge Mass Spectrometry (GDMS). Results confirmedthat the Ta ingot was 99.9992% pure.

Example 2

A potassium fluotantalate (K₂TaF₇) was obtained and upon spark sourcemass spec analysis, the K₂TaF₇ exhibited 5 ppm or less niobium. Levelsof Mo and W were also analyzed by spectrographic detection and levelswere below 5 ppm for Mo and below 100 ppm for W. In particular, theK₂TaF₇ had levels of Nb of 2 ppm or less, of Mo of less than 1 ppm andof W of less than or equal to 2 ppm. In each sample, the total recordedamount of Nb, Mo, and W was below 5 ppm. Four lots of 2,200 lbs. eachwere analyzed.

One of the lots was transferred to KDEL reactor which used a pure nickelvessel and a Hastelloy X agitator. The Hastelloy X agitator contained 9%Mo and 0.6% W. The shaft and paddles of the agitator were then shieldedwith {fraction (1/16)}″ nickel sheet using welding to clad all surfacesexposed to the reaction.

A standard sodium reduction process was used except as noted below. Thelot was subjected to the agitator in the presence of pure sodium to formtantalum powder. The tantalum powder was then washed with water andsubjected to acid treating and then steam drying and then screening to−100 mesh.

A sample from each batch was then submitted for glow discharge mass specanalysis. The two tables (Tables 1 and 2) below show the startinganalysis for the K₂TaF₇ and the final analysis of the tantalumrecovered.

TABLE 1 K₂TaF₇ Spark Source Mass Spec (SSMS) Analysis (metal to saltbasis) Sample Nb Mo W TOTAL Number (ppm) (ppm) (ppm) (ppm) 1 2 <1 ≦2 <52 1 <1 ≦2 <4 3 2 <1 ≦2 <5 4 1 <1 ≦2 <4

TABLE 2 Ta Powder Glow Discharge Mass Spec (GDMS) Analysis Sample Nb MoW TOTAL Number (ppm) (ppm) (ppm) (ppm) 5 1.4 0.38 0.27 2.05 6 1.2 0.300.50 2.00 7 1.0 0.25 0.29 1.54 8 1.1 0.15 0.28 1.53As can be seen in the above tables, a high purity tantalum powdersuitable for electron beam melting into an ingot can be obtained andpurities on the order of 99.999% purity can be obtained by theprocessing shown in Example 1.

Example 3

Two distinct process methodologies were used. First, a 99.998% puretantalum ingot was used which was subjected to three electron beamsmelts to produce a 12 inch nominal diameter ingot. The ingot wasmachined clean to about 11 ½ inch diameter and then heated in air toabout 260° C. for 4-8 hours. The ingot was then flat forged, cut, andmachined into slabs (approximately 4 inch by 10 inch with a length ofapproximately 28 inch to 32 inch) and then acid cleaned withHF/HNO₃/water solution. The slabs were annealed at 1050, 1150, and 1300°C. under vacuum of 5×10⁻⁴ Torr for 2 hours, then cold rolled into platestock of 0.500 and 0.250″ gauge. This cold rolling was accomplished bytaking a 4 inch thick by 10 inch wide by 30 inch long slab and rollingit perpendicular to the ingot axis at 0.200 inch per pass to 31 incheswide. The plate was then rolled parallel to the ingot axis at 0.100 inchper pass to 0.650 inch thick or 0.500 inch thick. Both rollings weredone on a 2-High breakdown rolling mill. Each of the plates were rolledby multiples passes of 0.050 inch per pass and then 0.025 inch per passwith final adjustments to meet a finish gauge of 0.500 inch plate or0.250 inch plate, using a four high finishing rolling mill. The plateswere then subjected to a final annealing at temperatures of from 950-1150° C.

The alternative process began with a 99.95% pure Ta which was subjectedto three electron beam melts to produce an ingot as described aboveprior to being forged. The ingot was then round forged using a GFMrotary forge to 4″ diameter after multiples passes of about 20%reduction in area per pass. From this intermediate stock, 4 billets(3.75″Ø×7″ long) were machined, and 2 billets (labeled A and B) wereannealed at 1050° C. while billets C and D remained unannealed. Next,the billets were upset forged to preforms of height of 2.5″, after whichpreforms A and C were annealed at 1050° C. The preforms were then clockrolled to a thickness of about 0.400″ to yield discs of a diameter ofapproximately 14″. This was accomplished by taking multiple passes of0.200 inch per pass to about 0.5250 inch thick. The discs were thenrolled to about 0.5 inch thick by multiple passes of 0.100 inch perpass. Then, the discs were clocked rolled on a four high finishing millin three passes of 0.050 inch, 0.025 inch, and 0.015 inch reductions perpass to yield a disc of about 0.400 inch thick by about 14 inchdiameter. A quarter of the disc was cut into four wedges and finalannealed at temperatures of 950-1100° C. Table 4 below summarizes thisprocessing.

Metallographic and texture analysis was conducted on longitudinalsections of the plate material (measurement face parallel to the finalrolling direction) and on radial sections of the forged and rolled discs(measurement face parallel to the radius of the discs).

Metallurgical Analysis

Grain size and texture were measured along the longitudinal or radialdirections of samples taken from rolled plate and forged and rolleddiscs, respectively. Grain size was measured using ASTM procedure E-112.Results from the annealing studies on products produced via the flat andround processes are given in Tables 3 and 4, respectively. Intermediateannealing treatments had no noticeable influence on the grain size ofthe finished product. Also, for plate, the final grain sizes of 0.500and 0.250″ thick tantalum were comparable. The only variable found tosignificantly effect the grain size of the materials was the finalanneal temperature: the higher the final anneal temperature, the largerthe resulting grain size.

In plate, grain sizes of ASTM 6.5-7.0 were measured in samples fromproduct annealed at 1000 and 950° C. However, each of these samplesshowed evidence of elongated and/or unrecrystallized regions at or nearthe surface, and recrystallization values were reported to be 98-99%.For plates annealed at 1050, 1100, and 1150° C., ASTM grain sizes rangedfrom 5.3 to 3.7, with all samples being 100% recrystallized.

For the round-processed discs, all samples were reported to be 100%recrystallized, with the exception of Disc C annealed at 950° C. whichwas 99% recrystallized. Grain sizes of ASTM 7.1-7.2, 6.1-6.8, and5.9-5.9 were measured in the disc samples annealed at 950, 1000, and1050° C., respectively. Annealing at 1100° C. produced grain sizes ofASTM 4.0-4.5.

For both processes, these findings demonstrate that a fullyrecrystallized grain size of 50 μm or finer is achievable using eitherthe plate rolling or the billet forging process at a preferred finalanneal temperature of from about 950 to about 1050° C. Should theunrecrystallized areas be limited to only the surface regions of theplate, then they can be removed by machining.

Texture Measurement Technique: A limited number of samples (chosen basedon metallurgical results) were used for texture analysis. Mounted andpolished samples, previously prepared for metallurgical analysis, wereemployed as texture samples after being given a heavy acid etch prior totexture measurement. Orientation Imaging Microscopy (OIM) was chosen asthe method of texture analysis because of its unique ability todetermine the orientation of individual grains within a polycrystallinesample. Established techniques such as X-ray or neutron diffractionwould have been unable to resolve any localized texture variationswithin the thickness of the tantalum materials.

For the analysis, each texture sample was incrementally scanned by anelectron beam (within an SEM) across its entire thickness; thebackscatter Kikuchi patters generated for each measurement point wasthen indexed using a computer to determine the crystal orientation. Fromeach sample, a raw-data file containing the orientations for each datapoint within the measurement grid array was created. These files servedas the input data for subsequently producing grain orientation maps andcalculating pole figures and orientation distribution functions (ODFs).

By convention, texture orientations are described in reference to thesample-normal coordinate system. That is, pole figures are“standardized” such that the origin is normal to the plate surface, andthe reference direction is the rolling (or radial) direction; likewise,ODFs are always defined with respect to the sample-normal coordinatesystem. Terminology such as “a (111) texture” means that the (111)atomic planes are preferentially oriented to be parallel (and the (111)pole oriented to be normal) with the surface of the plate. In theanalyses, the crystal orientations were measured with respect to thesample longitudinal direction. Therefore, it was necessary to transposethe orientation data from the longitudinal to sample-normal coordinatesystem as part of the subsequent texture analysis. These tasks wereconducted through use of computer algorithms.

Grain Orientation Maps: Derived from principles of presenting textureinformation in the form of inverse pole figures, orientation maps areimages of the microstructure within the sample where each individualgrain is “color-coded” based on its crystallographic orientationrelative to the normal direction of the plate of disc from which it wastaken. To produce these images, the crystal axes for each grain(determined along the longitudinal direction of the texture sample byOIM) were tilted 90° about the transverse direction so to align thecrystal axes to the normal direction of the sample. Orientation mapsserve to reveal the presence of texture bands or gradients through thethickness on the product; in tantalum, orientation maps have shown thatlarge, elongated grains identified by optical microscopy can be composedof several small grains with low-angle grain boundaries.

Analysis of the Texture Results: OIM scans were taken along thethickness of each sample provided; for the 0.500″ plate samples,separate measurements were made for the top and the bottom portions ofthe plate and reported separately.

The orientation maps were visually examined to qualitativelycharacterize the texture uniformity through the sample thickness. Toattain a quantifiable description of the texture gradients and texturebands in the example materials, the measured EBSD data was partitionedinto 20 subsets, with each representing a 5% increment of depth throughthe thickness of the sample. For each incremental data set, an ODF wasfirst calculated, then (100) and (111) centroid intensities determinednumerically using techniques reported elsewhere. The equipment andprocedures described in S. Matthies et al., Materials Science Forum,Vol. 157-162 (1994), pp. 1647-1652 and S. Matthies et al., MaterialsScience Forum, Vol. 157-162 (1994), pp. 1641-1646 were applied, andthese publications are incorporated in their entirety herein byreference. The texture gradients were then described graphically byplotting the (100) and (111) intensities, as well as the log ratio ofthe (100):(111), as a function depth of the sample. These results areset forth in FIGS. 1(A and B) through FIGS. 11(A and B).

The heavy-gauge tantalum plate exhibited the most uniformthrough-thickness texture; the only sample containing texture bands wasthat processed with a slab anneal of 1300° C. and a final anneal of1000° C. In addition, the 0.500″ plate materials also had a relativeweak (most random) texture base on pole figure and ODF analysis.Compared to the heavy plate, the 0.250′ sheets contained a slight tomoderate texture gradient and some evidence of texture banding. Also,the thin-gauge plates showed a more defined (111) texture in the ODFsand an increased prominence of (100).

The greatest variability in terms of texture uniformity and banding wasfound in the forged and rolled discs. Unlike the metallurgicalproperties, the texture of forged and rolled discs was effected by theuse of intermediate annealing. For discs A, B, and C, each of which wereprocessed with one or two intermediate annealing steps, the texturegradients ranged from negligible to strong (depending to processingparameters) with slight—if any—banding. However, for disc D, which wasworked from ingot to final discs without intermediate annealing, theresultant product contained less desirable strong texture gradients andsharp texture bands. Similarly, disc C, which was also forged fromunannealed billet but then annealed prior to cold rolling, also showed astrong texture gradient and banding in the sample final annealed at 950°C. For disc C, increasing the final anneal temperature to 1100° C. actedto diminish the gradient, eliminated the bands, but strengthening theintensity of (100) texture component. These effects from increasingfinal annealing temperatures were also evident, but to a lesser degree,in both the other disc materials and the heavy gauge plate.

From the microstructural and textural observations, the followingconclusions could be made regarding the optimum processing forfabricating tantalum sputtering targets:

-   -   For flat products, slab anneal temperatures preferably do not        exceed 1150° C. (1050° C. is more preferred) and the final        anneal temperature is preferably kept at 950-1000° C., more        preferably 1000° C. The resulting product is characterized as        having a recrystallized average grain size of less 50 μm. and        a (100) incremental intensity of less than 15 random and a log        ratio of (111):(100) of less than −4.0.    -   For round processing, billets preferably are annealed prior to        forging and rolling into disc without use of an intermediate        anneal at preform level. Final anneal temperature is preferably        950-1100° C., and more preferably is 1050° C. The resulting        product is characterized as having a recrystallized average        grain size below 50 μm, and a (100) incremental intensity of        less than 15 random and a log ratio of (111):(100) of less than        −4.0.

TABLE 3 Metallurgical Characteristics Process Slab Anneal Temperature (°C.) 1050 1150 1300 Gauge of Plate Produced from Slab .250¹¹ .500¹¹.250¹¹ .500¹¹ .250¹¹ .500¹¹ ASTM ASTM ASTM ASTM ASTM ASTM Grain % Grain% Grain % Grain % Grain % Grain % Plate Anneal Temperature (° C.) SizeRecry, Size Recry, Size Recry, Size Recry, Size Recry, Size Recry, 9507.0 98 6.7 98 7.0 98 6.7 98 7.0 98 6.7 98 1000 6.5 99 6.5 99 6.5 99 6.598 6.5 99 6.5 98 1050 4.5 100 5.0 100 4.5 100 5.0 99 4.5 100 5.3 1001050 5.0 100 4.5 100 5.0 100 4.5 100 5.0 100 4.5 100 1100 4.5 100 5.0100 4.5 100 4.0 100 4.5 100 4.0 100 1150 4.0 100 4.0 100 4.0 100 3.7 1004.0 100 3.7 100 Note: Material Purity was 99.998% Ta

TABLE 4 BILLET A BILLET B BILLET C BILLET D PC. WEIGHT Anneal 1050 C.Anneal 1050 C. Unannealed Unannealed 46.4 lbs 7″ Long Upset Forge UpsetForge Upset Forge Upset Forge 6.25″ 2.5″ Thick 2.5″ Thick 2.5″ Thick2.5″ Thick Diameter Anneal 1050 C. Anneal 1050 C. Machine MachineMachine Machine 42 lbs 6″ Diameter Clean Clean Clean Clean X-Roll toX-Roll to X-Roll to X-Roll to 15″ Gauge Gauge Gauge Gauge Diameter0.400″ 0.400″ 0.400″ 0.400″ Saw Cut Saw Cut Saw Cut Saw Cut 10.5lbs/qtr. Quarters Quarters Quarters Quarters Anneal Study Anneal StudyAnneal Study Anneal Study ANNEAL ASTM GRAIN TEMP(° C.) SIZE(REX)  9507.1 (100%) 7.2 (100%) 7.1 (99%)  7.2 (100%) 1000 6.1 (100%) 6.5 (100%)5.9 (100%) 6.8 (100%) 1050 5.8 (100%) 5.9 (100%) 5.9 (100%) 5.9 (100%)1100 4.5 (100%) 4.5 (100%) 4.5 (100%) 4.0 (100%) REX = %Recrystallization

Other embodiments of the present invention will be apparent to thoseskilled in the art from consideration of the present specification andpractice of the present invention disclosed herein. It is intended thatthe present specification and examples be considered as exemplary onlywith a true scope and spirit of the invention being indicated by thefollowing claims.

1. Tantalum metal having a purity of at last about 99.995% and anaverage grain size of about 75 microns or less.
 2. The tantalum metal ofclaim 1, wherein said metal is fully recrystallized.
 3. The tantalummetal of claim 1, wherein said metal is at least partiallyrecrystallized.
 4. A metal alloy comprising the tantalum metal of claim3.
 5. A sputtering target comprising the tantalum metal of claim
 3. 6. Acapacitor can comprising the tantalum metal of claim
 3. 7. A resistivefilm layer comprising the tantalum metal of claim
 3. 8. An articlecomprising at least as a component the tantalum metal of claim
 3. 9. Thetantalum metal of claim 1, wherein about 98% or more of said metal isrecrystallized.
 10. The tantalum metal of claim 1, wherein about 80% ormore of said metal is recrystallized.
 11. The tantalum metal of claim 1,wherein said metal has a) a texture in which a (100) pole figure has acenter peak intensity less than about 15 random or b) a log ratio of(111):(100) center peak intensities of greater than about −4.0, or c)both.
 12. The tantalum metal of claim 11, wherein said center peakintensity is from about 0 random to less than about 15 random.
 13. Thetantalum metal of claim 11, wherein said center peak intensity is fromabout 0 random to about 10 random.
 14. The tantalum metal of claim 11,wherein said log ratio is from greater than about −4.0 to about
 15. 15.The tantalum metal of claim 11, wherein said log ratio is from about−1.5 to about 7.0.
 16. The tantalum metal of claim 11, wherein saidcenter peak intensity is from about 0 random to less than about 15random, and said log ratio is from greater than about −4.0 to about 15.17. A metal alloy comprising the tantalum metal of claim
 11. 18. Asputtering target comprising the tantalum metal of claim
 11. 19. Acapacitor can comprising the tantalum metal of claim
 11. 20. A resistivefilm layer comprising the tantalum metal of claim
 11. 21. An articlecomprising at least as a component the tantalum metal of claim
 11. 22.The tantalum metal of claim 1 having a purity of from 99.995% to about99.999%.
 23. A metal alloy comprising the tantalum metal of claim
 1. 24.A sputtering target comprising the tantalum metal of claim
 1. 25. Acapacitor can comprising the tantalum metal of claim
 1. 26. A resistivefilm layer comprising the tantalum metal of claim
 1. 27. An articlecomprising at least as a component the tantalum metal of claim
 1. 28.The tantalum metal of claim 1, wherein the tantalum metal has asubstantially fine and uniform microstructure.
 29. The tantalum metal ofclaim 1, wherein the tantalum metal has an average grain size of fromabout 25 to about
 75. 30. The tantalum metal of claim 1, wherein saidaverage grain size is about 50 microns or less.
 31. A sputtering targetcomprising tantalum metal in the shape of a sputtering target having a)an average grain size of about 50 microns or less and b) a texture inwhich a log ratio of (111):(100) center peak intensities of greater thanabout −2.0, in the substantial absence of (100) textural bands, whereinsaid tantalum metal has a purity of at least 99.99% tantalum.
 32. Thesputtering target of claim 31 having an average grain size of from about25 to about 50 microns.
 33. The sputtering target of claim 31 having aratio of (111):(100) center peak intensities of greater than about 0.34. The sputtering target of claim 31, wherein said metal has a purityof at least 99.995% tantalum.
 35. The sputtering target of claim 34,wherein said metal is fully recrystallized.
 36. The sputtering target ofclaim 31, wherein said metal has a purity of 99.999% tantalum.
 37. Thesputtering target of claim 36, wherein said metal is fullyrecrystallized.
 38. The sputtering target of claim 31, wherein saidmetal is fully recrystallized.
 39. The sputtering target of claim 31,wherein about 80% or more of said metal is fully recrystallized.
 40. Thesputtering target of claim 31, wherein said log ratio is from about 0 toabout
 15. 41. Tantalum metal having a purity of a least about 99.995%,an average grain size of about 150 microns or less, and having a uniformprimary (111) texture through the thickness of the tantalum metal. 42.The tantalum metal of claim 41, wherein said metal is fullyrecrystallized.
 43. The tantalum metal of claim 41, wherein said metalis at least partially recrystallized.
 44. The tantalum metal of claim41, wherein about 98% or more of said metal is recrystallized.
 45. Thetantalum metal of claim 41, wherein about 80% or more of said metal isrecrystallized.
 46. The tantalum metal of claim 41, having a purity offrom 99.995% to about 99.999%.
 47. A sputtering target comprising thetantalum metal of claim
 41. 48. A capacitor can comprising the tantalummetal of claim
 41. 49. A resistive film layer comprising the tantalummetal of claim
 41. 50. An article comprising at least as a component thetantalum metal of claim
 41. 51. Tantalum metal having an average grainsize of about 75 or less, and having 50 ppm or less metallic impurities.52. The tantalum metal of claim 51, further having 50 ppm or less O₂, 25ppm or less N₂, or 25 ppm or less carbon, or combinations thereof. 53.The tantalum metal of claim 51, having 10 ppm or less metallicimpurities.
 54. The tantalum metal of claim 53, further having 50 ppm orless O₂, 25 ppm or less N₂, or 25 ppm or less carbon, or combinationsthereof.
 55. The tantalum metal of claim 51, wherein said average grainsize is about 50 microns or less.
 56. The tantalum metal of claim 51,where said average grain size is from about 25 to about 75 microns. 57.The tantalum metal of claim 51, wherein said metal is fullyrecrystallized.
 58. The tantalum metal of claim 51, wherein said metalis at least partially recrystallized.
 59. The tantalum metal of claim51, wherein about 98% or more of said metal is recrystallized.
 60. Thetantalum metal of claim 51, wherein about 80% or more of said metal isrecrystallized.
 61. The tantalum metal of claim 51, wherein said metalhas a) a texture in which a (100) pole figure has a center peakintensity less than about 15 random or b) a log ratio of (111):(100)center peak intensities of greater than about −4.0, or c) both.
 62. Thetantalum metal of claim 61, wherein said center peak intensity is fromabout 0random to less than about 15 random.
 63. The tantalum metal ofclaim 61, wherein said center peak intensity is from about 0 to about 10random.
 64. The tantalum metal of claim 61, wherein said log ratio isfrom greater than about 0 to about
 15. 65. The tantalum metal of claim61, wherein said log ratio is from about −1.5 to about 7.0.
 66. Thetantalum metal of claim 61, wherein said center peak intensity is fromabout 0 random to less than about 15 random, and said log ratio is fromgreater than about 4.0 to about
 15. 67. A sputtering target comprisingthe tantalum metal of claim
 51. 68. A capacitor can comprising thetantalum metal of claim
 51. 69. A resistive film layer comprising thetantalum metal of claim
 51. 70. An article comprising at least as acomponent the tantalum metal of claim
 51. 71. A tantalum sputteringcomponent comprising an average grain size of about 150 microns or lessand a uniform texture of primary (111) throughout a thickness of thecomponent, wherein said tantalum sputtering component comprises tantalumhaving a purity of at least 99.99% tantalum.
 72. The tantalum sputteringcomponent of claim 71, wherein said tantalum sputtering component is asputtering target.
 73. The tantalum sputtering component of claim 71,wherein said tantalum sputtering component has 50 ppm or less metallicimpurities.
 74. The tantalum sputtering component of claim 73, furtherhaving 50 ppm or less O₂, 25 ppm or less N₂, or 25 ppm or less carbon,or combinations thereof.
 75. The tantalum sputtering component of claim71, having 10 ppm or less metallic impurities.
 76. The tantalumsputtering component of claim 75, further having 50 ppm or less O₂, 25ppm or less N₂, or 25 ppm or less carbon, or combinations thereof.
 77. Asputtered deposited film of tantalum produced by the sputteringcomponent of claim
 71. 78. The tantalum sputtering component of claim71, wherein said average grain size is about 100 microns or less. 79.The tantalum sputtering component of claim 78, wherein said tantalumsputtering component is a sputtering target.
 80. The tantalum sputteringcomponent of claim 78, wherein said tantalum sputtering componentcomprises tantalum having a purity of at least 99.995% tantalum.
 81. Thetantalum sputtering component of claim 78, wherein said tantalumsputtering component comprises tantalum having a purity of at least99.999% tantalum.
 82. The tantalum sputtering component of claim 78,wherein about 98% or more of said tantalum sputtering component isrecrystallized.
 83. The tantalum sputtering component of claim 78,wherein about 80% or more of said tantalum sputtering component isrecrystallized.
 84. The tantalum sputtering component of claim 78,having a purity of from 99.995% to about 99,999%.
 85. The tantalumsputtering component of claim 78, further comprising a backing plate.86. The tantalum sputtering component of claim 71, wherein said tantalumsputtering component comprises tantalum having a purity of at least99.995% tantalum.
 87. The tantalum sputtering component of claim 71,wherein said tantalum sputtering component comprises tantalum having apurity of at least 99.999% tantalum.
 88. The tantalum sputteringcomponent of claim 71, wherein said tantalum sputtering component isfully recrystallized.
 89. The tantalum sputtering component of claim 71,wherein said tantalum sputtering component is at least partiallyrecrystallized.
 90. The tantalum sputtering component of claim 71,wherein about 98% or more of said tantalum sputtering component isrecrystallized.
 91. The tantalum sputtering component of claim 71,wherein about 80% or more of said tantalum sputtering component isrecrystallized.
 92. The tantalum sputtering component of claim 71 havinga purity of from 99.995% to about 99.9990%.
 93. The tantalum sputteringcomponent of claim 71, wherein said average grain size is about 50microns or less.
 94. The tantalum sputtering component of claim 71,wherein said average grain size is from about 25 to about 150 microns.95. The tantalum sputtering component of claim 71, wherein said averagegrain size is about 125 microns or less.
 96. The tantalum sputteringcomponent of claim 71, wherein said tantalum sputtering component isfully recrystallized.
 97. The tantalum sputtering component of claim 71,wherein said tantalum sputtering component is at least partiallyrecrystallized.
 98. The tantalum sputtering component of claim 71,further comprising a backing plate.
 99. A tantalum sputtering componentcomprising a uniform texture of primary (111) throughout a thickness ofthe component, wherein said tantalum sputtering component comprisestantalum having a purity of at least 99.99% tantalum.
 100. The tantalumsputtering component of claim 99, wherein said tantalum sputteringcomponent is a sputtering target.
 101. A sputtered deposited film oftantalum produced by a sputtering component of claim
 99. 102. Thetantalum sputtering component of claim 99, wherein said tantalumsputtering component comprises tantalum having a purity of at least99.995% tantalum.
 103. The tantalum sputtering component of claim 99,wherein said tantalum sputtering component comprises tantalum having apurity of at least 99.999% tantalum.
 104. The tantalum sputteringcomponent of claim 99, wherein said tantalum sputtering component isfully recrystallized.
 105. The tantalum sputtering component of claim99, further comprising a backing plate.
 106. A tantalum sputteringcomponent comprising an average grain size of about 75 microns or lessand a uniform texture of mixed (111) throughout its thickness, which issubstantially void of (100) textural bands, wherein said tantalumsputtering component comprises tantalum having a purity of at least99.99% tantalum.
 107. The tantalum sputtering component of claim 106,wherein said tantalum sputtering component is a sputtering target. 108.The tantalum sputtering component of claim 106, wherein said tantalumsputtering component comprises tantalum having a purity of at least99.995% tantalum.
 109. The tantalum sputtering component of claim 106,wherein said tantalum sputtering component comprises tantalum having apurity of at least 99.999% tantalum.
 110. The tantalum sputteringcomponent of claim 106, wherein said tantalum sputtering component isfully recrystallized.
 111. The tantalum sputtering component of claim106, wherein said tantalum sputtering component is at least partiallyrecrystallized.
 112. The tantalum sputtering component of claim 106,wherein about 98% or more of said tantalum sputtering component isrecrystallized.
 113. The tantalum sputtering component of claim 106,wherein about 80% or more of said tantalum sputtering component isrecrystallized.
 114. The tantalum sputtering component of claim 106,wherein said grain size is about 100 microns or less.
 115. The tantalumsputtering component of claim 106, wherein said grain size is about 50microns or less.
 116. The tantalum sputtering component of claim 106,wherein said average grain size is from about 25 to about 150 microns.117. The tantalum sputtering component of claim 106, further comprisinga backing plate.
 118. A tantalum sputtering component comprising a mixed(111) texture throughout its thickness which is substantially void of(100) textural bands wherein said tantalum sputtering componentcomprises tantalum having a purity of at least 99.99% tantalum.
 119. Thetantalum sputtering component of claim 118, wherein said tantalumsputtering component has an average grain size of about 150 microns orless.
 120. The tantalum sputtering component of claim 118, wherein saidaverage grain size is about 100 microns or less.
 121. The tantalumsputtering component of claim 118, wherein said tantalum sputteringcomponent is a sputtering target.
 122. The tantalum sputtering componentof claim 118, wherein said tantalum sputtering component comprisestantalum having a purity of at least 99.995% tantalum.
 123. The tantalumsputtering component of claim 118, wherein said tantalum sputteringcomponent comprises tantalum having a purity of at least 99.999%tantalum.
 124. The tantalum sputtering component of claim 118, whereinsaid tantalum sputtering component is fully recrystallized.
 125. Thetantalum sputtering component of claim 118, wherein said tantalumsputtering component is at least partially recrystallized.
 126. Thetantalum sputtering component of claim 118, wherein about 98% or more ofsaid tantalum sputtering component is recrystallized.
 127. The tantalumsputtering component of claim 118, wherein about 80% or more of saidtantalum sputtering component is recrystallized.
 128. The tantalumsputtering component of claim 118, wherein said average grain size isabout 50 microns or less.
 129. The tantalum sputtering component ofclaim 118, further comprising a backing plate.
 130. A tantalum sputtercomponent comprising an average grain size of about 75 microns or lessand a uniform texture of mixed (111) throughout its thickness, whereinsaid tantalum sputtering component comprises tantalum sputteringcomponent comprises tantalum having a purity of at least 99.99%tantalum.
 131. The tantalum sputter component of claim 130, wherein saidtantalum sputter component comprises tantalum having a purity of atleast 99.995% tantalum.
 132. The tantalum sputter component of claim130, wherein said tantalum sputter component comprises tantalum having apurity of at least 99.999% tantalum.
 133. The tantalum sputter componentof claim 130, wherein said tantalum sputter component comprises tantalumhaving a purity of from 99.995% to about 99.999.